硫铁矿烧渣水热法合成形貌可控的氧化铁

以硫铁矿烧渣硫酸浸出液与氨水反应制备的Fe(OH)3胶体为前驱体,采用水热法合成不同形貌的氧化铁粒子。在中性介质中考察反应温度、物质的量比(n(Fe2+)/n(Fe3+))、水热体系总Fe浓度及晶种量对水热法氧化铁物相、形貌和粒径的影响。采用X线衍射仪、扫描电镜、透射电镜及选择区域电子衍射对水热产物物相和形貌进行研究。研究结果表明:反应温度为230℃,n(Fe2+)/n(Fe3+)为0.1以及水热体系总Fe浓度为1.25 mol/L和晶种量为2 g时,水热产物为片状α-Fe2O3粒子;控制上述其他条件不变,当温度在140～260℃时,随着温度的升高,水热法产物由α-FeOOH相向α-Fe2O3相转变,α-Fe2O3粒子形貌由球形向小圆饼状和片状依次转变;当n(Fe2+)/n(Fe3+)在0～0.12时,随着n(Fe2+)/n(Fe3+)的增加,水热产物由α-Fe2O3相向α-Fe2O3和Fe3O4相转变,α-Fe2O3粒子形貌由球形逐渐向片状转变,其粒径由小变大;当水热体系中总Fe浓度为0.625 mol/L和1.875 mol/L时,水热法氧化铁分别为不均一形貌和球形;当没有加入晶种及晶种量为6 g时,水热...     

水热法制备CNTs/ZnS复合材料

在低温条件下利用水热法在未加修饰的原始碳纳米管(CNTs)上包覆硫化锌(ZnS)。利用X射线衍射(XRD)、场发射扫描电子显微镜(FE-SEM)和透射电子显微镜(TEM)测试表明ZnS层连续均匀的覆盖在CNTs上,厚度约为24 nm,具有闪锌矿结构,红外光谱结果说明乙酰胺吸附在CNTs/ZnS表面,抑制了ZnS层的厚度,紫外-可见吸收光谱结果表明在220 nm,265 nm处存在紫外吸收峰。以亚甲基蓝为目标降解物,光催化实验结果表明,与ZnS、CNTs相比,CNTs/ZnS复合材料显现出更好的光催化活性。     

基底预处理对于水热法制备ZnO微/纳米管阵列的影响

采用水热法系统研究了基底预处理(基底铺膜、不铺膜吹氮气处理和盐酸浸泡处理等)方式对于制备ZnO微/纳米管阵列的影响;结合ZnO晶体的微观结构,探讨了基底特征与ZnO微/纳米管阵列生长的内在联系.结果表明,采用高纯氮气和盐酸浸泡预处理基底均能制备得到ZnO微/纳米管阵列,并且这两种预处理方法制备出的纳米管在尺寸、形貌和分布上有所不同.ZnO微/纳米管成管机理研究表明,ZnO顶部锌终端对于生长微/纳米管起着决定性作用.     

可控电化学沉积制备纳米碳纤维电极

提出了一种简单制备纳米级碳纤维电极的新方法．微米级碳纤维经电化学刻蚀后，用循环伏安扫描法电化学沉积电泳漆，再经烘烤，绝缘漆固化收缩后露出纳米级的碳纤维尖端，通过再次电化学沉积可缩小电极面积，从而制得可控直径的纳米电极．该法可克服传统电泳漆固化后易留下小针孔的缺陷．用铁氰化钾溶液表征，确定了纳米碳纤维电极的有效面积，制得的纳米碳纤维电极的半径为几十到几百纳米。     

水热合成单分散碳球的制备与表征

以葡萄糖为原料水热法合成粒径均一单分散碳球,研究反应时间、反应温度、葡萄糖浓度、pH值、甲醛用量对碳球形貌及粒径的影响,采用SEM、FTIR、XRD对碳球的形貌和结构进行表征。结果表明,单分散碳球的最佳制备工艺为:反应温度160℃、反应时间6h、葡萄糖浓度0.25mol/L、体系pH值为8、甲醛用量2g;所制碳微球粒径约为350nm,分散系数为0.011,产率约为20%;制备出的碳球表面含有—OH、—CO、COOH官能团,碳球中含有无定形炭。     

Reduction-melting behaviors of boron-bearing iron concentrate/carbon composite pellets with addition of CaO

Although the total amount of boron resources in China is high, the grades of these resources are low. The authors have already proposed a new comprehensive utilization process of boron-bearing iron concentrate based on the iron nugget process. The present work de-scribes a further optimization of the conditions used in the previous study. The effects of CaO on the reduction–melting behavior and proper-ties of the boron-rich slag are presented. CaO improved the reduction of boron-bearing iron concentrate/carbon composite pellets when its content was less than 1wt%. Melting separation of the composite pellets became difficult with the CaO content increased. The sulfur content of the iron nugget gradually decreased from 0.16wt%to 0.046wt%as the CaO content of the pellets increased from 1wt%to 5wt%. CaO negatively affected the iron yield and boron extraction efficiency of the boron-rich slag. The mineral phase evolution of the boron-rich slag during the reduction–melting separation of the composite pellets with added CaO was also deduced.     

多孔TiO_2/FTO纳米有序阵列膜的可控生长研究

用脉冲激光沉积(PLD)技术在导电玻璃(FTO)衬底上沉积Ti膜,采用电化学阳极氧化方法,细致研究了FTO衬底上多孔TiO2纳米有序阵列膜的可控生长.结果表明,恰当的阳极电压对形成高度有序、孔径均匀的多孔TiO2/FTO阵列膜至关重要;通过优化的工艺参数,借助阳极氧化过程中各阶段电流-时间(I-t)曲线的准确判断,可实现对多孔TiO2阵列膜生长过程的有效控制,制备出高质量的多孔TiO2/FTO阵列膜.     

水热法碳化废旧棉织物制备碳微球的研究

利用废旧棉织物为原料,采用水热法在240~280℃温度范围下成功制备了碳微球。利用XRD、SEM和FT-IR对产物进行表征,通过ICP-Mas研究了产物对水中铝、铅等离子的吸附性能。从研究结果可知,水热反应温度为240~280℃,制备的碳微球粒径约为0.2~5.0μm,对铝、砷、镉、铅离子有较好的吸附性能。废旧棉织物在水热条件下发生水解、脱水,脱除有机基团过程中碳骨架发生球化趋势而逐渐成球。     

基于生物质甘蔗渣的荧光碳量子点制备

本实验以富含纤维素的废弃生物质甘蔗渣为原料,采用水热法合成了具有荧光性能的碳量子点.对碳量子点进行了表征,其粒径大小约为5~10 nm;在紫外灯照射下发蓝色荧光,对其荧光性能进行了研究,发现其具有多元激发、多元发射的性质.对其细胞毒性进行了研究,结果表明是一种生物相容性良好的标记材料.     

水热法制备碳纳米球修饰天然石墨材料CNS@NG

为改善石墨作为电极材料的性能,以葡萄糖和球形天然石墨为原料,采用水热法合成了碳纳米球修饰天然石墨材料CNS@NG。应用X射线衍射、扫描电子显微镜和拉曼光谱对样品的微观结构、形貌和组成进行表征。结果表明,由葡萄糖水热及碳化处理后形成的碳纳米球均匀地分布在球形天然石墨表面,所制备的合成材料样品较好地保持了天然石墨的晶体结构,表现出碳与石墨复合材料的拉曼特征,具有较好的稳定性。     

溶胶-水热法制备BaTiO3基PTC超细粉体

采用乙酸钡和钛酸四丁酯为原料,用溶胶沉淀与水热相结合的方法制备钛酸钡基正温度系数(PTC)纳米粉体.通过改变KOH强碱溶液用量调节水热反应的pH值,用X射线衍射分析了不同pH值条件下钛酸钡粉体晶相,确定了钛酸钡晶核稳定存在的条件.采用化学沉淀和溶液滴定方法研究了反应前驱物中Ba(AC)2和Ti(OC4H9)4的摩尔比对生成粉体化学计量比的影响.将Ba(AC)2Ti(OC4H9)4按照摩尔比为1配置的前驱物置于饱和氢氧化钡溶液构成的富钡环境下进行水热反应,获得了符合化学计量比、晶粒尺寸30nm左右的立方相钛酸钡纳米粉.在钛酸钡纯粉制备基础之上,将施主元素Y及受主元素Mn在前驱物制备过程中引入,瓷体实现了半导化,并获得了PTC效应.     

活化天然矿石选择性还原二氧化碳为无定形碳

Natural magnetite formed by the isomorphism substitutions of transition metals, including Fe, Ti, Co, etc., was activated by mechanical grinding followed by H₂ reduction. The temperature-programmed reduction of hydrogen (H₂-TPR) and temperature-programmed surface reaction of carbon dioxide (CO₂-TPSR) were carried out to investigate the processes of oxygen loss and CO₂ reduction. The samples were characterized by X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), and energy-dispersive X-ray spectroscopy (EDS). The results showed that the stability of spinel phases and oxygen-deficient degree significantly increased after natural magnetite was mechanically milled and reduced in H₂ atmosphere. Meanwhile, the activity and selectivity of CO₂ reduction into carbon were enhanced. The deposited carbon on the activated natural magnetite was confirmed as amorphous. The amount of carbon after CO₂ reduction at 300°C for 90 min over the activated natural magnetite was 2.87wt% higher than that over the natural magnetite.     

Selective reduction of carbon dioxide into amorphous carbon over activated natural magnetite

Natural magnetite formed by the isomorphism substitutions of transition metals, including Fe, Ti, Co, etc., was activated by mechanical grinding followed by H_2 reduction. The temperature-programmed reduction of hydrogen(H_2-TPR) and temperature-programmed surface reaction of carbon dioxide(CO_2-TPSR) were carried out to investigate the processes of oxygen loss and CO_2 reduction. The samples were characterized by X-ray diffraction(XRD), field emission scanning electron microscopy(FE-SEM), and energy-dispersive X-ray spectroscopy(EDS). The results showed that the stability of spinel phases and oxygen-deficient degree significantly increased after natural magnetite was mechanically milled and reduced in H_2 atmosphere. Meanwhile, the activity and selectivity of CO_2 reduction into carbon were enhanced. The deposited carbon on the activated natural magnetite was confirmed as amorphous. The amount of carbon after CO_2 reduction at 300°C for 90 min over the activated natural magnetite was 2.87 wt% higher than that over the natural magnetite.     

CaO/MgO和CaO/Ca9Al6O18吸收CO2的循环反应特性研究

钙基吸收剂是CO2捕集技术中常用的吸收剂,但随着循环次数的增加,天然钙基吸收剂循环反应特性下降明显.采用葡萄糖酸钙(Ca(C6H11O7)2)与葡萄糖酸镁(C12H22MgO14)及L-乳酸铝([CH3CH(OH)COO]3Al)作为前驱物,通过湿法混合的方法处理,制得了5种新型钙基吸收剂,试验研究了其吸收CO2的循环吸收能力及循环稳定性,分析了吸收剂组分、煅烧温度、煅烧气氛等条件对新型吸收剂循环反应特性的影响规律.研究结果表明,选用此前驱物制备的吸收剂,其循环反应特性明显高于传统的钙基吸收剂;其中,CaO/MgO(75wt%/25wt%)吸收剂具有最好的循环吸收能力,CaO/Ca9Al6O18(75wt%/wt25%)吸收剂具有最好的循环稳定性.通过研究煅烧条件对这两种吸收剂循环反应特性的影响,得到:850℃时,吸收剂表现出最佳的反应特性,而随着温度的升高,吸收剂的循环吸收能力有所下降;煅烧气氛对吸收剂循环吸收特性的影响与煅烧温度有显著的关系.     

Structural and mechanical properties of amorphous carbon films deposited by the dual plasma technique

Direct current metal filtered cathodic vacuum arc (FCVA) and acetylene gas (C₂H₂) were wielded to synthesize Ti-containing amorphous carbon films on Si (100). The influence of substrate bias voltage and acetylene gas on the microstructure and mechanical properties of the films were investigated. The results show that the phase of TiC in the (111) preferential crystallographic orientation exists in the film,and the main existing pattern of carbon is sp2. With increasing the acetylene flow rate,the contents of Ti and TiC phase of the film gradually reduce; however,the thickness of the film increases. When the substrate bias voltage reaches -600 V,the internal stress of the film reaches 1.6 GPa. The micro-hardness and elastic modulus of the film can reach 33.9 and 237.6 GPa,respectively,and the friction coefficient of the film is 0.25.     

水热法制备氧化锌纳米棒阵列的生长动力学研究

采用低温水热方法,在经预先修饰的基底上制备出取向高度一致的ZnO纳米棒阵列.用SEM和XRD等手段对制备的纳米棒阵列进行了表征.ZnO纳米棒阵列水热生长动力学表明:当生长时间在8 h内时,纳米棒的生长速度较快,之后纳米棒的生长近乎停止,棒的长度和直径基本不再改变.在生长速度较快的8 h内时,纳米棒的径向生长由两个明显的动力学过程组成,即由生长时间在1.5 h内的快速生长步骤和随后的慢速生长步骤组成;纳米棒的长度以约5.5 nm·min-1的生长速度增加至2.4 μm.     

气相生长碳纤维的制备

以苯和氢气为原料在石墨,陶瓷等基板表面催化热解制取低成本,高性能的气相生长碳纤维（ＶＧＣＦ）,实验考察了催化剂类热解温度、热解时间,苯带入量,载气,基板材料等参数对ＶＧＣＦ生长情况及性能的影响,并提出了碳纤维的生长机理。结果表明,在合适条件下,用直接播种法制得的ＶＧＣＦ直径为０．７￣１０μｍ,长度为１￣５μｍ,采用金属原子溅射沉积的基板可得到均匀稠密的ＶＧＣＦ,直径为３￣８０μｍ,碳纤维的生长过程     

炭纤维表面生长纳米碳管对CVI热解炭结构的影响

以单向长纤维预制体为骨架,CO为碳源,Ni为催化剂颗粒,在预制体炭纤维表面催化热解生长纳米碳管(CNT),采用CVI工艺增密,制得含CNT的C/C复合材料,研究纤维表面生长不同加载量的CNT对CVI过程所沉积热解炭微观结构的影响。研究结果表明:由于CNT具有特殊结构,纤维表面适当含量CNT能诱导CVI过程中热解炭的有序沉积,在近纤维层得到高织构度热解炭,改善炭纤维与热解炭的结合状态,拓宽制备粗糙层热解炭的CVI工艺条件范围;但当有过量CNT存在时,由于CNT之间的纠结,反而不利于发挥CNT对热解炭的催化诱导作用。     

水热条件下纳米羟基磷灰石的取向有序生长

为深入对骨组织中羟基磷灰石有序排列形成的了解,本研究采用水热条件结合模板法实现了羟基磷灰石纳米棒按一定的规律连生在一起,出现了取向连生现象.通过对其连生方式的分析发现了羟基磷灰石晶体在水热条件下生长存在各向异性,羟基磷灰石纳米棒在模板作用沿着其c轴易连生在一起.通过建立晶体生长过程模型,从而合理地解释了取向连生存在的规律性,为骨组织的仿生合成提供了理论基础.     

基底预处理对水热法制备SnO2纳米阵列生长的影响

采用水热法,在磁控溅射铺膜后的ITO-基底(MST-基底)上制备出取向一致的SnO2纳米线阵列.用X射线衍射(XRD)、扫描电子显微镜(SEM)、透射电子显微镜(TEM)和高分辨透射电子显微镜(HRTEM)等手段对制备的纳米线阵列进行了表征.考察了不同的基底铺膜方式和退火温度对产物形貌、尺寸和取向性的影响.结果表明,不同的基底铺膜方法对产物的形貌和尺寸有较大的影响:在磁控溅射法铺膜的基底上生长出SnO2纳米线阵列;在旋涂法铺膜的基底上生长出SnO2纳米棒阵列;在未铺膜基底上生长出SnO2纳米颗粒薄膜.另外,退火温度对生长在磁控溅射铺膜基底上的产物的取向性有较大的影响,随着退火温度的升高,产物的取向性增强.